CN102293804A - Optimized scheme for comprehensively utilizing silybum mariamum - Google Patents
Optimized scheme for comprehensively utilizing silybum mariamum Download PDFInfo
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- CN102293804A CN102293804A CN2010102093106A CN201010209310A CN102293804A CN 102293804 A CN102293804 A CN 102293804A CN 2010102093106 A CN2010102093106 A CN 2010102093106A CN 201010209310 A CN201010209310 A CN 201010209310A CN 102293804 A CN102293804 A CN 102293804A
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Abstract
The invention relates to the field of application of plant products, particularly an optimized scheme for comprehensively utilizing silybum mariamum. The invention solves the problems of poor comprehensive utilization effect of silybum mariamum, complex technique, high organic solvent consumption, low production efficiency, great potential safety hazard and the like, breaks through the restriction of the existing technical field; and the scheme of oil pressing after drying seeds extracted by ethanol simplifies the technique, enhances the production efficiency, improves the product quality, and is suitable for popularization.
Description
Technical field
The present invention relates to the application of vegetable products, is a kind of prioritization scheme of Herba Silybi mariani comprehensive utilization.
Background technology
Herba Silybi mariani is Compositae Silybum plant Silybum marianum (L.) Gaertner, and this plant originates in southern Europe, north African, and its seed extract " silymarin " at first is developed as treating hepatitis medicine (trade name: Legalon, sharp liver is grand) by Germany.This plant was introduced China in 1972, as a kind of medicinal plants popularizing planting that protects the liver.
The total flavones composition of silymarin (silymarin) for extracting in the Herba Silybi mariani seed, form by several flavanone kind compositions, main detection index components (content the strongest the highest, active composition) is silibinin (silybin A and B), and other has silidianin (silydianin), Silychristin (silychristin), silybonol (silybonol) etc.Silymarin is except that having anti-liver poisoning, protect liver plasma membrane, improving the liver function activity; clinical being used for the treatment of outside hepatitis, the cholecystitis; in recent years studies show that this composition still has anti peroxidation of lipid, radioprotective, removing free radical, antiulcer, blood fat reducing, prevents and treats atherosclerosis, prevention of brain ischemia, antiplatelet aggregation, anti-tumor activity, indicate that this composition becomes control cardiovascular and cerebrovascular disease and the good medicine of antineoplastic probably.It is reported that silibinin has entered I clinical trial phase (SinghRP, Agarwal R.Prostate cancer prevention by silibinin.Curr Cancer Drug Targets, 2004,4 (1): 1-11) of treatment carcinoma of prostate.That studies gos deep into the expansion of application, the demand market of having opened silymarin.
China introduces silymarin from nineteen eighty-three from Germany and extracts production line, and annual output total amount in the whole nation also had only about 20 tons at that time, and mainly as the raw material of homemade new drug silybin, manufacturer has 85 families in by the end of January, 2005 by.Yet difficulty because the maturation time of Herba Silybi mariani seed differs, gathers, have again to extract and adopted a large amount of inflammable and explosive organic solvents, production security is poor, cause developed countries such as America and Europe, Japan based on buying silymarin crude product raw material, carry out retrofit, preparing product is sold various countries then and is raked in enormous profits.Estimate according to the parties concerned, China's silymarin year total volume of exports surpasses more than 300 tons at present, entered silymarin export trade big country ranks, product is found a good sale in the U.S., Canada, Belgium, Britain, Philippine, Japan, Korea S, India, Australia and tens countries and regions such as China Hong Kong, Taiwan.
Though China is silymarin production, big export country, continued to use the traditional processing technology (following diagram) of the eighties in last century substantially.Investigation finds that domestic utilization to Herba Silybi mariani at present mainly is to extract silymarin, is auxilliary to seed medium oil and proteic extraction and application.At first squeeze oil, gained oil can be used as edible oil after refining.Grouts after the oil expression continue with the defat of petroleum ether equal solvent, dewaxing, carry out hot reflux with ethyl acetate, acetone again and extract, and extracting solution promptly gets the silymarin crude product after reclaiming solvent, seldom have producer that it is proceeded purification.Remaining contain the solvent grouts behind desolventizing as feedstuff or directly make fertilizer and use.
Above-mentioned traditional handicraft has the following disadvantages:
1) when oil squeezing system,, and make in the oil pigment many because of partial pigment in the seed hulls is brought into;
2) grouts after the oil expression, with petroleum ether or gasoline defat a few hours, the time is long, consumption of organic solvent is big, and is inflammable and explosive usually;
3) extract silymarin and adopt ethyl acetate, acetone equal solvent, extracting cycle is long, solvent loss is big, and needs the residual of control solvent in the finished product;
4) silymarin of Sheng Chaning still belongs to crude product, and wherein main pharmacodynamics composition silibinin A and B sum are lower than 20%;
5) residue behind the extraction silymarin needs to remove residual solvent, carries out the processing of proteic preparation or feedstuff again.
In recent years, because the consumer of the U.S., Europe, Japan is more and more stricter for the requirement of residual quantities such as solvent acetone, ethyl acetate, petroleum ether, this product and price thereof to outlet producer is a challenge greatly.According to distributors, present homemade silymarin price is 70 dollars/kilogram, and Italy produces 110 dollars/kilogram of silymarin, and its quality gap is self-evident.
Summary of the invention
An object of the present invention is to solving in the above-mentioned prior art technology of extracting silymarin when the squeezing system oil,, and make in the oil pigment many because of partial pigment in the seed hulls is brought into; Grouts after the oil expression, with petroleum ether or gasoline defat, the time is long, consumption of organic solvent is big, and is inflammable and explosive usually; Extract silymarin and adopt ethyl acetate, acetone equal solvent, extracting cycle is long, solvent loss is big, and needs the residual of control solvent in the finished product; The silymarin of production is of poor quality, and the residue behind the extraction silymarin needs to remove residual solvent, carries out the processing of proteic preparation or feedstuff again, problems such as complex process, the prioritization scheme that provides a kind of Herba Silybi mariani to fully utilize.
For achieving the above object, a technical scheme of the present invention provides a kind of prioritization scheme of Herba Silybi mariani comprehensive utilization, and this scheme comprises the steps:
At first be to adopt edible ethanol that the Herba Silybi mariani seed is extracted, extract obtains silymarin through resin absorption roguing, purification; Row oil expression again behind the seed drying behind the ethanol extraction; Oil expression gained grouts are directly used in preparation albumen or processing feedstuff.
Included step is elaborated as follows:
1) gets ripe Herba Silybi mariani seed, screen out silt; To clean the Herba Silybi mariani seed and drop into extraction pot, and add ethanol, preferred edible ethanol extracts more than 2 times, generally extracts 3 times and can farthest extract silymarin;
Preferred version: adopt 4-12 doubly to measure 40-90% edible ethanol reflux, extract, more than 2 times, each extraction time is more than the 1hr.;
More preferably scheme: add 8,6,6 times of amount 60-80% edible ethanol reflux, extract, three times respectively, the time is respectively 2hr.1.5hr., 1.5hr., and preferred alcohol concentration is 60-80%;
2) extracting solution is merged, concentrating under reduced pressure reclaims ethanol; Preferred version: reclaim ethanol to containing alcohol amount 15-20%;
3) above-mentioned liquid through with the resin absorption of quality of medicinal material 1: 0.5-2, the absorption flow velocity is 1.2-2.5BV/hr.; Preferred version: above-mentioned liquid warp and 1: 1 resin absorption of quality of medicinal material, the absorption flow velocity is 1.5-2BV/hr.;
4) resin column after the absorption is through the roguing of 2-4BV deionized water eluting;
5) resin column after the roguing, through the edible ethanol desorption silymarin of 50-90%, the desorption flow velocity is 1-1.5BV/hr., preferred concentration of alcohol is 60-80%;
6) the desorbing attached liquid, cools off to there not being the alcohol flavor through decompression recycling ethanol, and silymarin is isolated in centrifugal filtration, through deionized water wash, promptly gets silymarin;
Also comprise drying steps, the silymarin filter cake is pulverized in 50-70 ℃ of vacuum drying, packing; Seed behind ethanol extraction volatilizes residual ethanol, and oil expression makes Herba Silybi mariani oil, and pigment is few in the oil, is a kind of health care oil of high value; Grouts can prepare albumen or be machined directly to feedstuff to be sold.
Described adsorbent resin, in a large amount of resins of different manufacturers, different model, the polarity that filters out after deliberation, strong Polar Adsorbent Resin, preferred HPD-600, LSA-7, ADS-7, XDA-8.
Beneficial effect of the present invention is: two guest's content (the HPLC method mensuration) 25-50% of Herba Silybi mariani in the silymarin, and traditional handicraft less than 20% (referring to patent CN 101381363A, a kind of method of extracting macroporous adsorption resin and separating hepadestal from alkaline water).
Grouts in the traditional handicraft after oil expression must be earlier clean with oil stain removing before extracting silymarin, otherwise remaining oils and fats can influence the extraction of silymarin.The inventor did experiment: if directly extract with ethyl acetate, acetone equal solvent without defat the oil expression back, then influence the quality and the productive rate of silymarin.For solving acetone equal solvent residue problem in the silymarin product, the inventor also once attempted, adopt conventional process, the oil expression grouts extract silymarin after defat, with tradition extract solvent ethyl acetate, acetone is replaced by edible ethanol, impurity such as the small-molecular peptides that exists in the discovery seed, albumen just are extracted, and influence the quality of silymarin product equally.In a word, silymarin is extracted in the traditional handicraft defat again of extracting oil earlier then, and technology is numerous and jumbled, yields poorly, and is of poor quality, and dissolvent residual is difficult for removing; The present invention has broken away from the thought binding in the prior art field, has adopted the method for first extraction silymarin.Extract silymarin, prepare albumen or processing feedstuff then with seed oil expression, grouts after extracting again with edible ethanol.So just exempt the grouts necessary petroleum ether/gasoline skimming processes before extracting silymarin after traditional handicraft is extracted oil.Extract silymarin with edible ethanol, can avoid solvent (acetone, ethyl acetate) residual, proposed by ethanol because of the partial pigment in kind of the shell simultaneously, also reduced residual (see embodiment) of pigment in squeezing Herba Silybi mariani oil.
The present invention is owing to adopted the prioritization scheme of comprehensive utilization, get rid of the step that adopts petroleum ether or gasoline defat, solved problems such as degreasing time is long, consumption of organic solvent is big, and is inflammable and explosive, accelerated production, enhance productivity, reduce cost, also reduced the potential safety hazard in the production process simultaneously, and, by the prioritization scheme of comprehensive utilization process, also can reduce employed equipment accordingly, reduce cost from the aspect of production equipment.Below only will extract silymarin and adopt traditional handicraft and optimization improvement technology to be compared as follows, be beneficial to raising the efficiency, reduce cost, improve the understanding of production security.
| Method | Degreasing solvent | Extract solvent | Consuming time to extract silymarin |
| Traditional method | 120# gasoline | Ethyl acetate | 120# gasoline defat 3-4 time, (2BV, 3hr.)/time, meter 9-12hr.; Ethyl acetate (2.5BV, 2BV, 2BV) is extracted 3 times, 4hr./time, No. 3 meter 12hr..Amount to 20-24hr. |
| Optimization method | ---- | Edible ethanol | 70% edible ethanol is extracted (8BV, 2hr. 3 times; 6BV, 1.5hr.; 6BV, 1.5hr.), meter 5hr. |
[0032]Annotate: solvent load is for extracting the multiple of raw materials quality in the table.Traditional method is organized volume referring to " comprehensive utilization of Herba Silybi mariani " editor. " comprehensive utilization of Herba Silybi mariani ", Beijing: Science Press, 1980:52-61
The present invention adopts edible ethanol as solvent, surplus materials behind the preparation silymarin does not need again through painstakingly removing the processing of solvent, simplified production stage, reduce cost, simultaneously also avoided processing by traditional handicraft, not thorough because of removal of solvents, residue after the extraction is made feedstuff and the toxic and side effects that produces, or makes problems such as can causing adverse effect in the proteic process.
Silibinin A and Herba Silybi mariani B content in the silymarin that the present invention program makes (HPLC method mensuration) are 25-50%, and traditional handicraft then is lower than 20%.
Figure of description
Fig. 1 is a flow chart of the present invention
Fig. 2 is the flow chart of existing scheme that conventional art adopts
The specific embodiment
Further specify the present invention below in conjunction with embodiment, but not as a limitation of the invention.
Embodiment 1
Herba Silybi mariani seed 250Kg adds 75% edible ethanol 2000L, and heating and refluxing extraction 2hr. filters.Filtering residue is added with 2000L, 1300L and distinguishes reflux, extract, twice again, each 1.5hr..Merge ethanol extract.Residue goes alcohol dry back oil expression, and grouts are for preparation albumen or processing feedstuff.
Ethanol extract is through an amount of solvent of reclaim under reduced pressure, with the 1.5-2BV/hr. velocity flow through 300Kg Polar Adsorbent Resin HPD-600, after with deionized water flush away impurity, press 1-1.5BV/hr. speed eluting object with 5-6BV70% ethanol again, eluent does not have the alcohol flavor through being evaporated to, centrifugal filtration, and centrifugal thing is through 60 ℃ of drying under reduced pressure, pulverizing, promptly get silymarin 4.25Kg, HPLC detects the two guests (A and B) 33% of Herba Silybi mariani.
Embodiment 2:
Herba Silybi mariani seed 300Kg adds 75% edible ethanol 2400L, and heating and refluxing extraction 2hr. filters.Filtering residue is added with 1800L, 1800L and distinguishes reflux, extract, twice again, each 1.5hr..Merge ethanol extract.Residue goes alcohol dry back oil expression, and grouts are for preparation albumen or processing feedstuff.
Ethanol extract is extremely an amount of through decompression and solvent recovery, with the 1.5-2BV/hr. velocity flow through 300Kg Polar Adsorbent Resin ADS-7, after with deionized water flush away impurity, press 1-1.5BV/hr. speed eluting object with 5-6BV70% ethanol again, eluent does not have the alcohol flavor through being evaporated to, centrifugal filtration, and centrifugal thing is through 60 ℃ of drying under reduced pressure, pulverizing, promptly get silymarin 5.75Kg, HPLC detects the two guests (A and B) 31% of Herba Silybi mariani.
Embodiment 3:
Herba Silybi mariani seed 250Kg adds 80% edible ethanol 2000L, and heating and refluxing extraction 2hr. filters.Filtering residue is added with 1500L, 1500L and distinguishes reflux, extract, twice again, each 1.5hr..Merge ethanol extract.Residue goes alcohol dry back oil expression, and grouts are for preparation albumen or processing feedstuff.
Ethanol extract is extremely an amount of through decompression and solvent recovery, with the 1.5-2BV/hr. velocity flow through 250Kg Polar Adsorbent Resin LSA-7, after with deionized water flush away impurity, press 1-1.5BV/hr. speed eluting object with 5-6BV75% ethanol again, eluent does not have the alcohol flavor through being evaporated to, centrifugal filtration, and centrifugal thing is through 60 ℃ of drying under reduced pressure, pulverizing, promptly get silymarin 4.31Kg, HPLC detects the two guests (A and B) 31.6% of Herba Silybi mariani.
Embodiment 4:
Herba Silybi mariani seed 300Kg adds 70% edible ethanol 2400L, and heating and refluxing extraction 2hr. filters.Filtering residue is added with 1800L, 1800L and distinguishes reflux, extract, twice again, each 1.5hr..Merge ethanol extract.Residue goes alcohol dry back oil expression, and grouts are for preparation albumen or processing feedstuff.
Ethanol extract is extremely an amount of through decompression and solvent recovery, with the 1.5-2BV/hr. velocity flow through 300Kg Polar Adsorbent Resin XDA-8, after with deionized water flush away impurity, press 1-1.5BV/hr. speed eluting object with 5-6BV70% ethanol again, eluent does not have the alcohol flavor through being evaporated to, centrifugal filtration, and centrifugal thing is through 60 ℃ of drying under reduced pressure, pulverizing, promptly get silymarin 5.55Kg, HPLC detects the two guests (A and B) 32% of Herba Silybi mariani.
Embodiment 5
The Herba Silybi mariani cast of oil relatively.Tradition is squeezed Herba Silybi mariani oil and the Herba Silybi mariani oil of improving one's methods and squeezing, with the Lab method that is widely used in various food color difference analysis at present (the Li Lite work. physical properties of food. Beijing, Chinese agriculture publishing house, 1998:323-331) determination data is as follows:
| Product | L-value |
| Improve technology Herba Silybi mariani oil | 20.86 |
| Traditional handicraft Herba Silybi mariani oil | 20.12 |
Annotate: L-value is big, shows that the product color is light, transparency good.
Claims (9)
1. the prioritization scheme of a Herba Silybi mariani comprehensive utilization is characterized in that, with ethanol the Herba Silybi mariani seed is extracted, and extract obtains silymarin through resin absorption roguing, purification; Row oil expression again behind the seed drying behind the ethanol extraction.
2. according to the prioritization scheme of the described Herba Silybi mariani of claim 1 comprehensive utilization, it is characterized in that describedly with ethanol the Herba Silybi mariani seed is extracted, extract is through resin absorption roguing, purification, the detailed process that obtains silymarin is as follows:
(1) gets ripe Herba Silybi mariani seed, screen out silt; To clean the Herba Silybi mariani seed and drop into extraction pot, add ethanol, extract more than 2 times;
(2) extracting solution is merged, concentrating under reduced pressure reclaims ethanol;
(3) above-mentioned liquid through with quality of medicinal material than 1: the resin absorption of 0.5-2, the absorption flow velocity is 1.2-2.5BV/hr.;
(4) resin column after the absorption is with the roguing of deionized water eluting;
(5) resin column after the roguing, through the edible ethanol desorption silymarin of 50-90%,
(6) the desorbing attached liquid is through decompression recycling ethanol, and silymarin is isolated in cooling, through deionized water wash, promptly gets silymarin.
3. according to the prioritization scheme of the described Herba Silybi mariani comprehensive utilization of claim 2, it is characterized in that,
Described step (1) is doubly measured 40-90% edible ethanol reflux, extract, more than 2 times for adopting 4-12, and each extraction time is more than the 1hr.;
Reclaim ethanol in the described step (2) to containing alcohol amount 15-20%;
Through the liquid and 1: 1 the resin absorption of medical material amount of ethanol extraction, the absorption flow velocity is 1.5-2BV/hr. in the described step (3);
The eluting roguing is through the roguing of 2-4BV deionized water eluting in the described step (4);
It is the alcoholic solution desorption of 60-80% that described step (5) is selected concentration for use, and flow velocity is 1-1.5BV/hr.;
The desorbing attached liquid to there not being the alcohol flavor, is isolated silymarin through decompression recycling ethanol in the described step (6) after the centrifugal filtration, through deionized water wash, promptly gets silymarin.
4. according to the prioritization scheme of the described Herba Silybi mariani comprehensive utilization of claim 3, it is characterized in that described step (1) is for adding 8,6,6 times of amount 60-80% edible ethanol reflux, extract, three times respectively, the time is respectively 2hr., 1.5hr., 1.5hr..
5. according to the prioritization scheme of the arbitrary described Herba Silybi mariani comprehensive utilization of claim 2-4, it is characterized in that, also comprise drying steps, the silymarin filter cake is pulverized in 50-70 ℃ of vacuum drying, packing.
6. according to the prioritization scheme of the arbitrary described Herba Silybi mariani comprehensive utilization of claim 1-4, it is characterized in that described adsorbent resin is selected from polarity or strong polar resin.
7. according to the prioritization scheme of the described Herba Silybi mariani of claim 6 comprehensive utilization, it is characterized in that, described adsorbent resin is selected among HPD-600 (Hebei Bao En resin processing plant), ADS-7 (Tianjin Nankai with become company), LSA-7, the XDA-8 (Xi'an Lan Xiao company) any one.
8. according to the prioritization scheme of the arbitrary described Herba Silybi mariani comprehensive utilization of claim 1-4, it is characterized in that the seed behind ethanol extraction volatilizes residual ethanol, oil expression makes Herba Silybi mariani oil;
9. according to the prioritization scheme of the arbitrary described Herba Silybi mariani comprehensive utilization of claim 1-4, it is characterized in that, extract silymarin and oil expression back gained grouts, be used to prepare albumen or processing feedstuff.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104450172A (en) * | 2014-12-10 | 2015-03-25 | 江苏中兴药业有限公司 | Fructussilybi oil extraction method |
| CN104650050A (en) * | 2014-01-17 | 2015-05-27 | 吴长军 | Method for extracting silymarin by using food-grade ethanol as an extracting solvent |
| CN108740383A (en) * | 2018-06-13 | 2018-11-06 | 河南全赫饲料有限公司 | A kind of sheep fattening particle batch and preparation method thereof |
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| CN1560046A (en) * | 2004-03-03 | 2005-01-05 | 西安理工大学 | Process for extracting water grind thisvine using alcohole as single organic dissolvent |
| CN101381363A (en) * | 2007-09-06 | 2009-03-11 | 天津大学 | Method for extracting macroporous adsorption resin and separating hepadestal from alkaline water |
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| CN1560046A (en) * | 2004-03-03 | 2005-01-05 | 西安理工大学 | Process for extracting water grind thisvine using alcohole as single organic dissolvent |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104650050A (en) * | 2014-01-17 | 2015-05-27 | 吴长军 | Method for extracting silymarin by using food-grade ethanol as an extracting solvent |
| CN104650050B (en) * | 2014-01-17 | 2019-03-15 | 吴长军 | It is a kind of with the silymarin extracting method that food grade ethyl alcohol is Extraction solvent |
| CN104450172A (en) * | 2014-12-10 | 2015-03-25 | 江苏中兴药业有限公司 | Fructussilybi oil extraction method |
| CN108740383A (en) * | 2018-06-13 | 2018-11-06 | 河南全赫饲料有限公司 | A kind of sheep fattening particle batch and preparation method thereof |
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